Method and composition for pulse dose cleaning of process streams

ABSTRACT

Pulse dosing is used to administer a cleaning formulation into a fluid process stream flowing through structural components of a processing facility. The fluid process stream may contain corn, corn-derived products, or a combination thereof, or the fluid process stream may contain a process condensate, a rinse fluid, a cleaning fluid or any combination thereof. The processing facility may be an ethanol processing plant, a protein processing plant, a corn oil processing plant, an ethanol and corn oil processing plant, an ethanol and protein processing plant, or an ethanol, corn oil and protein processing plant. Pulse dosing may include administering the cleaning formulation into the fluid process stream for a period of x seconds every y minutes, with no administration of the cleaning formulation between the periods of x seconds.

CROSS-REFERENCE TO RELATED APPLICATIONS

This application is a continuation of U.S. application Ser. No.17/158,900, filed Jan. 26, 2021, which claims the benefit of the earlierfiling date of U.S. Provisional Application No. 62/966,338, filed Jan.27, 2020, each of which is incorporated by reference in its entiretyherein.

FIELD

This disclosure concerns a method for using pulse dosing to administer acleaning formulation into a fluid process stream flowing throughstructural components of a processing facility.

BACKGROUND

Ethanol, protein, dry distillers grain, and/or oil processing plantstypically use a cleaning in place (CIP) approach to controlling depositbuildups and bacteria that negatively impact ethanol, corn oil, andprotein production. CIP events require plants to shut down sections ofthe plant periodically while it is still running to clean. These eventsrequire significant labor input and use of cleaning chemicals. CIPevents also typically reduce plant efficiency while the cleaning cycleis ongoing since the section of the plant being cleaned is eitherpartially or completely inoperable during the cleaning event. Methodsfor enhancing cleaning and yields of processing streams are needed inthe art.

SUMMARY

Embodiments of a method for using pulse dosing to administer a cleaningformulation into a fluid process stream flowing through structuralcomponents of a processing facility are disclosed. Embodiments ofcleaning formulations also are disclosed.

Embodiments of the disclosed method include using pulse dosing toadminister a cleaning formulation into a fluid process stream flowingthrough structural components of a processing facility, the fluidprocess stream comprising (i) corn, corn-derived products, or acombination thereof, or (ii) a process condensate, a rinse fluid, acleaning fluid, or any combination thereof. In some embodiments, pulsedosing comprises administering the cleaning formulation into the fluidprocess stream for a period of x seconds every y minutes, with noadministration of the cleaning formulation between the periods of xseconds, wherein x and y independently are from 1 to 500. In any of theforegoing or following embodiments, an amount of the cleaningformulation administered into the fluid process stream may provide aconcentration of 10 ppm to 50,000 ppm of the cleaning formulation in thefluid process stream during the period of x seconds. In any of theforegoing or following embodiments,

In any of the foregoing or following embodiments, the processingfacility may be an ethanol processing plant, a protein processing plant,a corn oil processing plant, an ethanol and corn oil processing plant,an ethanol and protein processing plant, or an ethanol, corn oil andprotein processing plant. In some embodiments, the processing facilitycomprises one or more structural components selected from a heating andliquefaction unit, a heat exchanger unit, a propagation unit, afermentation unit, a distillation unit, an evaporation unit, acentrifuge unit, a fiber separation unit, a protein separation unit, anoil separation unit, or any combination thereof. In some embodiments,the cleaning formulation is administered into the fluid process streamat, or upstream of, at least one of the one or more structuralcomponents.

In any of the foregoing or following embodiments, pulse dosing may beperformed at each of two or more of the structural components of theprocessing facility for a period of x seconds every y minutes, with noadministration of the cleaning formulation between the periods of xseconds at each of the two or more structural components, wherein each xand y independently is from 1 to 500. In some embodiments, an amount ofthe cleaning formulation administered into the fluid process stream ateach of the two or more structural components independently provides aconcentration of 10 ppm to 50,000 ppm of the cleaning formulation in thefluid process stream.

In some embodiments, the fluid process stream comprises corn,corn-derived products, or a combination thereof, and (i) the cleaningformulation is administered into, or upstream of, the heating andliquefaction unit, and a mean pressure increase over time within theheating and liquefaction unit is smaller than a mean pressure increaseover time when the cleaning formulation is not administered using pulsedosing; or (ii) the cleaning formulation is administered into, orupstream of, the heat exchange unit, and a mean pressure increase overtime within the heat exchange unit is smaller than a mean pressureincrease over time when the cleaning formulation is not administeredusing pulse dosing; or (iii) the cleaning formulation is administeredinto, or upstream of, the heating and liquefaction unit, and a meantemperature drop over time within the heating and liquefaction unit issmaller than a mean temperature drop over time when the cleaningformulation is not administered using pulse dosing; or (iv) the cleaningformulation is administered into, or upstream of, the heat exchangerunit, and a mean temperature drop over time within the heat exchangerunit is smaller than a mean temperature drop over time when the cleaningformulation is not administered using pulse dosing; or (v) the cleaningformulation is administered into, or upstream of, the fiber separationunit, and a mean flow rate over a period of time through the fiberseparation unit is greater than a mean flow rate over the period of timethrough the fiber separation unit when the cleaning formulation is notadministered using pulse dosing; or (vi) the cleaning formulation isadministered into, or upstream of, the protein separation unit, and amean flow rate over a period of time through the protein separation unitis greater than a mean flow rate over the period of time through theprotein separation unit when the cleaning formulation is notadministered using pulse dosing; or (vii) the cleaning formulation isadministered into, or upstream of, the oil separation unit, and a meanflow rate and/or oil production over a period of time through the oilseparation unit is greater than a mean flow/or oil production over theperiod of time through the oil separation unit when the cleaningformulation is not administered using pulse dosing; or (viii) anycombination of (i)-(vii).

In some embodiments, the fluid process stream comprises a processcondensate, rinse fluid, or combination thereof, and the method furtherincludes ceasing flow of a product process stream comprisingcorn-derived products through at least one of the one or more structuralcomponents; initiating flow of the fluid process stream comprising theprocess condensate, rinse fluid, or combination thereof through the atleast one of the one or more structural components; and using pulsedosing to administer the cleaning formulation into the fluid processstream comprising the process condensate, rinse fluid, or combinationthereof. In certain embodiments, (i) pulse dosing comprisesadministering the cleaning formulation into the fluid process streamcomprising the process condensate, rinse fluid, or combination thereoffor a period of x seconds every y minutes, with no administration of thecleaning formulation between the periods of x seconds, wherein x and yindependently are from 1 to 500; or (ii) an amount of the cleaningformulation is administered into the fluid process stream comprising theprocess condensate, rinse fluid, or combination thereof to provide aconcentration of 10 ppm to 50,000 ppm of the cleaning formulation in thefluid process stream during the period of x seconds; or (iii) both (i)and (ii).

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is a block diagram of certain components and/or steps involved inan exemplary ethanol and oil processing plant.

FIG. 2 is a photographic image of an evaporator tube prior to cleaning.

FIG. 3 is a photographic image of the evaporator tube of FIG. 2 aftercleaning with a cleaning formulation comprising nitric acid and adetergent using a standard CIP process.

FIG. 4 is a photographic image of a screen cleaned with asurfactant-based formulation and a caustic.

FIG. 5 is a photographic image of a screen cleaned with a caustic onlyusing a standard CIP process.

FIG. 6 is a graph showing effects of pulse dose administration of acleaning formulation to a mash bank on the ratio of pressure to flowrate over time as the fluid process stream flowed from the mash bank tothe fermentation unit.

FIG. 7 is a photographic image of an oil separator unit disc followingpulse dosing with a cleaning formulation administered to the fluidprocess stream.

FIG. 8 is a photographic image of oil separator unit discs followingpulse dosing with a cleaning formulation administered to the fluidprocess stream and rinsing with a standard pressure washer.

FIG. 9 is a graph showing effects of pulse dose administration of acleaning formulation at doses of 0, 500, and 1000 ppm on flow ratethrough a secondary screen of a fiber separation unit.

FIG. 10 is a graph showing effects of pulse dose administration of acleaning formulation at doses of 0, 500, and 1000 ppm on flow ratethrough a secondary screen of a fiber separation unit.

FIG. 11 is a graph showing flow rates over time through primary,secondary, and tertiary screens of a fiber separation unit in theabsence of pulse dose administration of a cleaning formulation.

FIG. 12 is a graph showing flow rates over time through primary,secondary, and tertiary screens of a fiber separation unit with pulsedose administration of a cleaning formulation.

FIGS. 13A and 13B are graphs showing change in pressure over time(dP/dt) in a mash bank in the presence or absence of pulse doseadministration of a cleaning formulation.

FIGS. 14A and 14B are graphs showing change in temperature over time(dT/dt) in a mash bank in the presence or absence of pulse doseadministration of a cleaning formulation.

FIGS. 15A and 15B are graphs showing change in pressure over time(dP/dt) in a mash bank in the presence or absence of continuous low-doseadministration of the cleaning formulation of FIGS. 13A-13B.

FIGS. 16A and 16B are graphs showing change in temperature over time(dT/dt) in a mash bank in the presence or absence of continuous low-doseadministration of a cleaning formulation of FIGS. 14A-14B.

FIGS. 17A-170 are graphs showing effects of pulse dose administration ofa cleaning formulation at doses of 0, 500, and 2000 ppm at a secondaryscreen of a fiber separation unit on flow rate through the secondaryscreen.

FIGS. 18A-18B are graphs showing effects of continuous low-doseadministration of the cleaning formulation to a primary screen of afiber separation unit on flow rate through the primary screen.

FIGS. 19A-19B are graphs showing effects of continuous low-doseadministration of the cleaning formulation to a secondary screen of afiber separation unit on flow rate through the secondary screen.

FIGS. 20A-20B are graphs showing effects of continuous low-doseadministration of the cleaning formulation to a tertiary screen of afiber separation unit on flow rate through the tertiary screen.

DETAILED DESCRIPTION

Embodiments of a method for using pulse dosing to administer a cleaningformulation into a fluid process stream flowing through structuralcomponents of a processing facility are disclosed. In some embodiments,the fluid process stream comprises corn, corn-derived products, or acombination thereof. The fluid process stream may include, but is notlimited to, mash, whole stillage and thin stillage. In some embodiments,the fluid process stream comprises a process condensate, a rinse fluid,a cleaning fluid, or any combination thereof. The process condensate maybe, for example, condensate from an evaporation unit. Exemplaryprocessing facilities include ethanol, protein, dry distillers grain,and/or corn oil processing plants. In some embodiments, the processingfacility is an ethanol processing plant, a protein processing plant, acorn oil processing plant, an ethanol and corn oil processing plant, anethanol and protein processing plant, or an ethanol, corn oil andprotein processing plant.

I. Explanation of Terms

The following explanations of terms and abbreviations are provided tobetter describe the present disclosure and to guide those of ordinaryskill in the art in the practice of the present disclosure. As usedherein, “comprising” means “including” and the singular forms “a” or“an” or “the” include plural references unless the context clearlydictates otherwise. The term “or” refers to a single element of statedalternative elements or a combination of two or more elements, unlessthe context clearly indicates otherwise.

Unless explained otherwise, all technical and scientific terms usedherein have the same meaning as commonly understood to one of ordinaryskill in the art to which this disclosure belongs. Although methods andmaterials similar or equivalent to those described herein can be used inthe practice or testing of the present disclosure, suitable methods andmaterials are described below. The materials, methods, and examples areillustrative only and not intended to be limiting. Other features of thedisclosure are apparent from the following detailed description and theclaims.

Although the steps of some of the disclosed methods are described in aparticular, sequential order for convenient presentation, it should beunderstood that this manner of description encompasses rearrangement,unless a particular ordering is required by specific language set forthbelow. For example, steps described sequentially may in some cases berearranged or performed concurrently. Additionally, the descriptionsometimes uses terms like “produce” and “provide” to describe thedisclosed methods. These terms are high-level abstractions of the actualsteps that are performed. The actual steps that correspond to theseterms will vary depending on the particular implementation and arereadily discernible by one of ordinary skill in the art.

Unless otherwise indicated, all numbers expressing quantities ofcomponents, molecular weights, percentages, temperatures, times, and soforth, as used in the specification or claims are to be understood asbeing modified by the term “about.” Accordingly, unless otherwiseindicated, implicitly or explicitly, the numerical parameters set forthare approximations that may depend on the desired properties soughtand/or limits of detection under standard test conditions/methods. Whendirectly and explicitly distinguishing embodiments from discussed priorart, the embodiment numbers are not approximates unless the word “about”is recited. Furthermore, not all alternatives recited herein areequivalents.

Detergent: A substance that reduces the surface tension of water.Specifically, a surface-active agent, or surfactant, that concentratesat oil-water interfaces and exerts an emulsifying action. Detergents areclassified as anionic, cationic, or nonionic, depending on their mode ofchemical action. Nonionic detergents function via a hydrogen-bondingmechanism.

Downstream: As used herein, the term “downstream” refers to a pointanywhere in the fluid process stream after a site (e.g., after astructural component) where a cleaning formulation is administered.Immediately downstream means a downstream point in the fluid processstream that is proximate the administration site.

Pulse dosing: Intermittent dosing, i.e., periods of dosing alternatingwith periods of no dosing.

Scale: A hard mineral coating or corrosion deposit composted of solidsand sediments that collect on components in a processing facility as aprocess stream flows through or over the components.

Surfactant: A compound that reduces surface tension when dissolved inwater or water solutions, or that reduces interfacial tension betweentwo liquids. A surfactant molecule typically has a polar or ionic “head”and a nonpolar hydrocarbon “tail.” Upon dissolution in water, thesurfactant molecules aggregate and form micelles, in which the nonpolartails are oriented inward and the polar or ionic heads are orientedoutward toward the aqueous environment. Micelles typically are sphericalin shape and small, with diameters of less than about 10 nm. Thenonpolar tails create a nonpolar “pocket” within the micelle.

Upstream: When referring to the flow of a fluid process stream into astructural component, the term “upstream” refers to a point anywhere inthe fluid process stream prior to entering the structural component. Forexample, upstream of an evaporator refers to any point in the fluidprocess stream before the fluid process stream flows through theevaporator. Immediately upstream means a point in the fluid processstream proximate entry into the structural component. With referenceagain to an evaporator, immediately upstream refers to a point in thefluid process stream just before it enters the evaporator and after ithas flowed through all structural components located prior to theevaporator in the process.

II. Introduction

Continuous dosing of cleaning formulations into a process stream is amethod used in processing plants of various industries to reduce foulingand/or bacterial contamination, thereby reducing frequency of facilityshut-downs for cleaning. However, effective dosing levels for thesetypes of formulations may not be practical or economical on a continuousdose basis. As disclosed herein, pulse dosing effectively controlsdeposit and bacteria formation in the plant while achieving theseoutcomes at an economically feasible cost and with reduced consumptionof the cleaning formulations. At least some advantages of this approachto ethanol plants and other industries include, but are not limited to,(i) more efficient production of ethanol, oil, and protein; (ii) longertimes between cleaning cycles, and/or (iii) less challenging cleaningevents, providing significant maintenance savings in labor and cleaningchemicals.

In some of the disclosed implementations, the processing plant is anethanol processing plant, a protein processing plant, an oil processingplant, an ethanol and oil processing plant, an ethanol and proteinprocessing plant, or an ethanol, oil and protein processing plant. Theoil may be corn oil. The process stream may be a fluid process streamcomprising (i) corn, corn-derived products, or a combination thereof, or(ii) a process condensate, a rinse fluid, a cleaning fluid, or anycombination thereof. In some embodiments, the fluid process streamincludes, but is not limited to, mash, whole stillage and thin stillage.In some implementations, the process stream comprises a processcondensate.

In some embodiments, a processing facility comprises one or morestructural components selected from a milling unit, a heating/cookingand liquefaction unit, a heat exchanger unit (also referred to as a mashbank), a propagation unit (e.g., for propagating yeast), a fermentationunit, a distillation unit, an evaporation unit, a centrifuge unit, afiber separation unit, a protein separation unit, an oil separationunit, or any combination thereof. Each unit may comprise one or morecomponents arranged in series or in parallel. For instance, adistillation unit may comprise one, two, three, or more distillationcolumns. An evaporation unit may comprise, one, two, three, or moreevaporators. A fiber separation unit may comprise a plurality ofseparation screens; for instance, the fiber separation unit maysequentially comprise primary, secondary, and tertiary separationscreens.

A block diagram of one exemplary corn-to-ethanol processing facility 100is shown in FIG. 1 , which shows certain structural components and/orsteps involved in corn-to-ethanol processing. Although the diagram ofFIG. 1 shows one exemplary arrangement of the facility components, aperson of ordinary skill in the art will understand that otherarrangements are also possible and the exemplary arrangement of FIG. 1is not necessarily preferred. The processing facility 100 includes amilling unit 101 where corn is milled to form a corn mash or fluidprocess stream. The milled corn process stream flows through a cookingunit 102 and a liquefaction unit 103, in which the corn mash is cookedand degraded into its component parts, e.g., fiber, protein, oils, etc.In some processing facilities, the process stream then flows through afiber separation unit 104 and a protein separation unit, which removefiber and protein, respectively, from the fluid process stream. In otherprocessing facilities, the process stream flows directly from theliquefaction unit 103 to the fermentation unit 106. Although theexemplary arrangement of FIG. 1 shows fiber separation prior to proteinseparation, the person of ordinary skill in the art understands,particularly with the benefit of the present disclosure, that proteinseparation can be performed prior to fiber separation if desired oreither process can be performed on its own. The fluid process streamthen flows into the fermentation unit 106 where the fluid process streamis fermented to produce ethanol. The fermented fluid process streamflows into the distillation unit 107, which may comprise one or moredistillation columns. Ethanol is distilled from the process stream, andthe remainder of the process stream flows into the centrifuge 108,wherein solids are separated from the fluid process stream. The fluidprocess stream is then split, with part of the stream being recycledback to cooking unit 102 and part of the stream flowing to an evaporatorunit 109, wherein low molecular-weight components, e.g. water and othervolatile components, are removed from the fluid process stream,providing a fluid stream comprising a syrup. The syrup then flows intothe oil separation unit 110, which separates corn oil from any remainingsolids that formed in the evaporator unit 109. Although not shownexplicitly, the person of ordinary skill in the art understands,particularly with the benefit of the present disclosure, that thecooking unit 102, liquefaction unit 103, fermentation unit 106,distillation unit 107, and/or evaporator unit 109 may comprise one ormore heat exchangers.

III. Pulse Dosing Method

Disclosed herein are embodiments of a pulse dosing method foradministering cleaning formulations into process streams, includingcorn-to-ethanol process streams as discussed herein. Formulationembodiments that can be used in such methods are described herein.

The disclosed method uses pulse dosing to administer a cleaningformulation into a fluid process stream flowing through structuralcomponents of a processing facility. In some embodiments, the fluidprocess stream comprises (i) corn, corn-derived products, or acombination thereof, or (ii) a process condensate, a rinse fluid, acleaning fluid, or any combination thereof. In any of the foregoing orfollowing embodiments, the cleaning formulation may comprise adetergent, an organic deposit control formulation, a scale inhibitor, apH modifier, an oxidizer, a caustic solution or any combination thereof.

In any of the foregoing or following embodiments, pulse dosing maycomprise administering the cleaning formulation into the fluid processstream for a period of x seconds every y minutes, with no administrationof the cleaning formulation between the periods of x seconds. In someembodiments, x and y independently are from 1 to 500, such as 1-250,1-150, 5-150, 5-100, 10-100, 10-90, 15-90, or 15-60. In certainexamples, x and y independently are 5, 10, 15, 30, 45, 60, or 90. Insome non-limiting examples, the cleaning formulation is pulse dosed intothe fluid process stream for a period of 5 seconds every 5 minutes, 10seconds every 10 minutes, 15 seconds every 15 minutes, 30 seconds every30 minutes, 45 seconds every 45 minutes, 60 seconds every 60 minutes, or90 seconds every 90 minutes. In any of the foregoing or followingembodiments, x and y may be the same or different. In some embodiments,x and y are the same, e.g., 30 seconds every 30 minutes. In someembodiments, x and y are different, e.g., 15 seconds every 30 minutes or45 seconds every 30 minutes.

Administering the cleaning formulation into the process stream via pulsedosing may be performed by any suitable method. In some embodiments,administering is performed by flowing, injecting, or spraying thecleaning formulation into the fluid process stream. Administration maybe performed at a continuous or substantially continuous rate throughouteach period of x seconds. The amount of cleaning formulationadministered is selected to provide a desired concentration in the fluidprocess stream. In some embodiments, the cleaning formulation is a fluidand a volume sufficient to provide a desired concentration isadministered into the fluid process stream over each period of xseconds.

In any of the foregoing or following embodiments, the cleaningformulation may be pulse dosed into the fluid process stream to provideany desired or effective concentration of the cleaning formulation inthe fluid process stream during the period of x seconds. In someembodiments, the cleaning formulation is pulse dosed into the fluidprocess stream to provide a concentration of 10 ppm to 50,000 ppm of thecleaning formulation in the fluid process stream during the period of xseconds. The concentration may be determined at or immediatelydownstream of the site where the cleaning formulation is administered.In some embodiments, the concentration is 10 ppm to 25,000 ppm, 15 ppmto 20,000 ppm 20 ppm to 15,000 ppm, 50 ppm to 10,000 ppm, 100 ppm to5,000 ppm, 100 ppm to 2,000 ppm, 125 ppm to 2000 ppm, 250 ppm to 2000ppm, 250 ppm to 1500 ppm, 250 ppm to 1000 ppm, or 250 ppm to 750 ppm.The processing facility may be an ethanol processing plant, a proteinprocessing plant, a corn oil processing plant, an ethanol and corn oilprocessing plant, an ethanol and protein processing plant, or anethanol, corn oil and protein processing plant. In some embodiments, theprocessing facility comprises one or more structural components selectedfrom a heating and liquefaction unit, a heat exchanger unit, apropagation unit, a fermentation unit, a distillation unit, anevaporation unit, a centrifuge unit, a fiber separation unit, a proteinseparation unit, an oil separation unit, or any combination thereof, aspreviously described. The cleaning formulation may be administered intothe fluid process stream in, or upstream of, at least one of the one ormore units using pulse dosing. In some embodiments, the cleaningformulation is administered into the fluid process stream in, orupstream of, the heating and liquefaction unit, the heat exchanger unit,the evaporation unit, the fiber separation unit, the protein separationunit, the oil separation unit, or any combination thereof.

In any of the foregoing or following embodiments, pulse dosing may beperformed at different stages of the process. For example, a cleaningformulation may be administered via pulse dosing into the fluid processstream in, or upstream of, two or more of the processing facilitystructural components. The cleaning formulations administered into thefluid process stream at each of the two or more structural componentsmay have the same chemical composition or cleaning formulations withdifferent chemical compositions may be administered at each of the twoor more structural components. For instance, an organic deposit controlformulation may be administered into the fluid process stream at a firststructural component, and a scale inhibitor formulation may beadministered into the fluid process stream at a subsequent structuralcomponent. In any of the foregoing or following embodiments, the pulsedosing may be performed at each of the two or more structural componentsfor a period of x seconds every y minutes, with no administration of thecleaning formulation between the periods of x seconds at each of the twoor more structural components, wherein each x and y independently isfrom 1 to 500, such as 1-250, 1-150, 5-150, 5-100, 10-100, 10-90, 15-90,or 15-60. In certain examples, x and y independently are 15, 30, 45, 60,or 90. In some embodiments, x=y at each one of the two or morestructural components, e.g., 60 seconds every 60 minutes. In otherembodiments, x #y, e.g., 20 seconds every 30 minutes. In someembodiments, x and y are the same at a given structural component, butmay differ from structural component to structural component within theprocessing facility. For instance, pulse dosing may be performed for 30seconds every 30 minutes at a first structural component, and for 60seconds every 60 minutes at a subsequent structural component. In someimplementations, x and y are the same at each of the two or morestructural component. For example, pulse dosing may be performed for 30seconds every 30 minutes at each of the two or more structuralcomponents. Additionally, an amount of cleaning formulation administeredvia pulse dosing to each of the two or more structural componentsindependently provides a concentration of 10 ppm to 50,000 ppm of thecleaning formulation in the fluid process stream. In some embodiments,the concentration at each of the two or more structural componentsindependently is 10 ppm to 25,000 ppm, 15 ppm to 20,000 ppm, 20 ppm to15,000 ppm, 50 ppm to 10,000 ppm, 100 ppm to 5,000 ppm, 100 ppm to 2,000ppm, 125 ppm to 2000 ppm, 250 ppm to 2000 ppm, 250 ppm to 1500 ppm, 250ppm to 1000 ppm, or 250 ppm to 750 ppm. For instance, in onenon-limiting example, the cleaning formulation may be administered tothe heat exchanger unit for 30 seconds every 30 minutes to provide aconcentration of 250 ppm in the fluid process stream at or immediatelydownstream of the heat exchanger unit, and also may be administered tothe fiber separation unit for 30 seconds every 30 minutes to provide aconcentration of 500 ppm in the fluid process stream at or immediatelydownstream of the fiber separation unit.

In another example, the fiber separation unit may comprise one or moreseparation screens, and the cleaning formulation is administered intothe fluid process stream via pulse dosing upstream of at least one ofthe one or more of the separation screens. In one embodiment, the fiberseparation unit comprises a primary separation screen, a secondaryseparation screen, and a tertiary separation screen. In this embodiment,the cleaning formulation is administered into the fluid process streamvia pulse dosing at the secondary separation screen to provide a firstconcentration of the cleaning formulation in the fluid process stream ator proximate the secondary separation screen, and the cleaningformulation is administered into the fluid process stream via pulsedosing at the tertiary separation screen to provide a secondconcentration of the cleaning formulation in the fluid process stream ator proximate the tertiary separation screen. In some implementations,the second concentration is less than the first concentration. Forinstance, the first concentration may be 500 ppm and the secondconcentration may be 250 ppm, or the first concentration may be 750 ppm,and the second concentration may be 500 ppm or 250 ppm. Additionally,each pulse dosing interval (x and y, as described herein) at each screenmay be the same or different. In one implementation, the pulse dosingintervals at the secondary and tertiary screens are the same such thatthe cleaning formulation is dosed to into the fluid process stream ateach of the secondary and tertiary screens for 30 seconds every 30minutes.

In some embodiments, the fluid process stream comprises corn,corn-derived products, or a combination thereof, and pulse dosing thecleaning formulation into the fluid process stream at mash banks(heating and liquefaction units) and heat exchangers can improve heattransfer efficiency, which provides energy savings, as well as controlof bacterial buildup in the mash banks that can impact fermentationfurther downstream, leading to less bacteria (and more ethanol) andextending time between CIP cleaning cycles. Metrics associated with suchembodiments can include delta pressure, delta temperature, in beer, andmash flows. In some implementations, the cleaning formulation isadministered via pulse dosing into, or upstream of, the heating andliquefaction unit, and a mean pressure increase and/or temperature dropover time within the heating and liquefaction unit is smaller than amean pressure increase and/or temperature drop over time when thecleaning formulation is not administered using pulse dosing. In someimplementations, the cleaning formulation is pulse dosed into, orupstream of, the heat exchange unit, and a mean pressure increase and/ortemperature drop over time within the heat exchange unit is smaller thana mean drop pressure increase and/or temperature drop over time when thecleaning formulation is not administered using pulse dosing as describedherein. For instance, the mean pressure increase and/or temperature dropover time may be smaller than a mean drop in pressure and/or temperaturewhen (i) no cleaning formulation is administered, and/or (ii) anequivalent low dose of the cleaning formulation is continuouslyadministered, i.e., an amount of the cleaning formulation iscontinuously added to the fluid process stream to provide a constant orsubstantially constant concentration (e.g., a concentration varying byno more than ±10% relative to an average concentration). Continuousadministration may be performed at a single point within the processingfacility, e.g., into or upstream of the heating or liquefaction unit, orupstream of the fiber separation unit. An equivalent low dose isdetermined by calculating the dose that would be provided if the pulsedose is instead continuously administered; that is, pulse dosing toprovide a cleaning formulation concentration of 500 ppm in the fluidprocess stream for 60 seconds every 60 minutes is equivalent tocontinuously administering to provide a constant or substantiallyconstant cleaning formulation concentration of 8.3 ppm in the fluidprocess stream. In certain examples, the mean pressure increase overtime at a given structural component of the processing facility is atleast 1% smaller, at least 2% smaller, at least 5% smaller or at least10% smaller than the mean pressure increase when the cleaningformulation is not administered using pulse dosing. Pressure increasesas deposits build up on the structural component(s) and restrict flow ofthe fluid process stream. Pulse dosing effectively reduces the rate ofdeposit formation and thus reduces the rate at which pressure increasesat the structural component. The mean pressure increase over time undera pulse dosing regimen may be 1-20%, 2-20%, 5-20%, or 10-15% smallerthan the mean pressure increase over time in the absence of pulsedosing. In some examples, the mean temperature drop over time is atleast 1% smaller, at least 2% smaller, at least 5% smaller, at least 10%smaller than the mean temperature drop over time when the cleaningformulation is not administered using pulse dosing. As deposits build upon structural components, the temperature drops over time. Temperaturedrops may be attributed to reduced flow rate and/or restricted heattransfer due to the deposits. The mean temperature drop under a pulsedosing regimen may be 1-15%, 2-15%, 5-15%, or 10-15% smaller than themean temperature drop in the absence of pulse dosing.

In some embodiments, cleaning formulation that is pulse dosed into afluid process stream comprising corn, corn-derived products, or acombination thereof, at mash banks will flow subsequently into apropagator, removing deposits and bacteria that negatively impactethanol production, and extending time between CIP cleaning cycles. Inadditional embodiments, cleaning formulation that is dosed into thefluid process stream at the mash banks will flow into the fermentationfill headers, removing deposits and bacteria that negatively impactethanol production extending time between CIP cycles and improvingethanol production efficiency. Metrics associated with such embodimentscan include lactic acid delta (change in lactic acid values over time)and acetic acid delta.

In yet some additional embodiments, cleaning formulation that is pulsedosed into the mash banks will flow into the fermentation, deliveringcorn mash that has lower bacteria populations that negatively impactethanol production, thereby extending time between CIP cleaning cyclesand providing improved ethanol production efficiency. Metrics associatedwith such embodiments can include lactic acid delta and acetic aciddelta.

In some embodiments, pulse dosing the cleaning formulation into a fluidprocess stream comprising corn, corn-derived products, or a combinationthereof at the evaporators to control deposit buildup can be used toimprove heat transfer and evaporation efficiency and extending timebetween CIP cleaning cycles. Metrics associated with such embodimentscan include steam use, efficiency, and 1St and 2nd effect pressures.

In yet some additional embodiments, cleaning formulation that is pulsedosed into the fluid process stream at the evaporators will flowdownstream to the oil recovery system, removing deposits on oilseparation equipment, thereby providing increased oil production andextending time between CIP cleaning cycles. Metrics associated with suchembodiments can include flow rate through the oil separation unit andaveraged oil production. In some implementations, the cleaningformulation is administered via pulse dosing into, or upstream of, theoil separation unit, and a mean flow rate over a period of time throughthe oil separation unit is greater than a mean flow rate over the periodof time through the oil separation unit when the cleaning formulation isnot administered using pulse dosing. For instance, the mean flow ratemay be greater and/or may drop more slowly than a flow rate when (i) nocleaning formulation is administered, and/or (ii) an equivalent low doseof the cleaning formulation is continuously administered. The flow ratethrough the oil separation unit under a pulse dosing regimen may be atleast 0.1% greater, at least 0.2% greater, or at least 0.3% greater thanan average flow rate through the oil separation unit in the absence ofpulse dosing. The flow rate under a pulse dosing regimen may be 0.1-10%,0.1-5%, or 0.1-2% greater than the flow rate in the absence of pulsedosing. The increased flow rate may be attributed to a reduced amount ofdeposits forming on structural components of the processing facility,thereby producing less restricted flow through conduits, separationscreens, and/or other structural components through which the processstream flows. A person of ordinary skill in the art understands thatflow rate can also be increased by the plant independently of any impactof pulse dosing.

In some embodiments, using pulse dosing to administer the cleaningformulation into a fluid process stream comprising corn, corn-derivedproducts, or a combination thereof, at, or immediately upstream of,separation screens that separate corn fiber from the protein andfermentable portions of corn can be used to improve separationefficiency and thereby extending time between CIP cleaning cycles. Or,using pulse dosing to administer the cleaning formulation into the fluidprocess stream at the protein separation clarifier can be used toimprove protein production efficiency, thereby extending time betweenCIP cleaning cycles. Metrics associated with such embodiments caninclude the flow rate, time between cleanings, and/or proteinproduction. In some implementations, the cleaning formulation is pulsedosed into the fluid process stream at, or upstream of, the fiberseparation unit (or upstream of one or more of a plurality of separationscreens of the separation unit), and a mean flow rate over a period oftime through the fiber separation unit is greater than a mean flow rateover the period of time through the fiber separation unit when thecleaning formulation is not administered using pulse dosing. In someimplementations, the cleaning formulation is pulse dosed into the fluidprocess stream at, or upstream of, the protein separation unit, and amean flow rate over a period of time through the protein separation unitis greater than a mean flow rate over the period of time through theprotein separation unit when the cleaning formulation is notadministered using pulse dosing. For instance, the mean flow rate may begreater and/or may drop more slowly than a flow rate when (i) nocleaning formulation is administered, and/or (ii) an equivalent low doseof the cleaning formulation is continuously administered. The flow ratethrough the fiber separation unit and/or protein separation unit under apulse dosing regimen may be at least 0.1% greater, at least 0.2%greater, or at least 0.3% greater than an average flow rate through thefiber separation unit and/or protein separation unit in the absence ofpulse dosing. The flow rate under a pulse dosing regimen may be 0.1-10%,0.1-5%, or 0.1-2% greater than the flow rate in the absence of pulsedosing.

In some embodiments, the fluid process stream comprises a processcondensate, a rinse fluid, a cleaning fluid, or any combination thereof,and pulse dosing is used as part of a CIP process. The processcondensate may be obtained, for example, from an evaporator unit of theprocessing facility. The process condensate may comprise water and otherlow molecular weight, volatile components. In some implementations, arinse fluid comprises water or an aqueous buffered solution.

In some embodiments, a CIP process includes ceasing flow of a productprocess stream comprising corn-derived products through at least one ofthe one or more structural components of the processing facility,initiating flow of the fluid process stream comprising the processcondensate, rinse fluid, or combination thereof through the at least oneof the one or more structural components, and using pulse dosing toadminister the cleaning formulation into the fluid process streamcomprising the process condensate, rinse fluid, or combination thereof.In certain embodiments, pulse dosing comprises administering thecleaning formulation into the fluid process stream comprising theprocess condensate, rinse fluid, or combination thereof for a period ofx seconds every y minutes, with no administration of the cleaningformulation between the periods of x seconds, wherein x and yindependently are from 1 to 500. Frequently, the values of x and yin aCIP process in which the process stream comprises a process condensateand/or a rinse fluid are greater than the values of x and y used whenthe process stream is a product process stream comprising corn,corn-derived products, or a combination thereof. For instance, in someembodiments of a CIP process, the cleaning formulation is added for aperiod of 60-300 seconds every 350-900 minutes. In certain embodimentsof the CIP process, x #y.

In any of the foregoing or following embodiments, an amount of thecleaning formulation may be administered into the fluid process streamcomprising the process condensate, rinse fluid, or combination thereofto provide a concentration of 10 ppm to 50,000 ppm of the cleaningformulation in the fluid process stream during the period of x seconds.In any of the foregoing or following embodiments, the cleaningformulation may comprise a detergent, an organic deposit controlformulation, a scale inhibitor, a pH modifier, an oxidizer, a causticsolution, or any combination thereof.

In some embodiments, a CIP process comprises a first stage and a secondstage. Pulse dosing as described herein may be used in either stage ofthe CIP process. In some embodiments, the first stage can compriseadding a surfactant-based detergent cleaning formulation to a processstream wherein the cleaning formulation (e.g., an amount to provide aconcentration of 500 ppm) is added to a process condensate pre-rinse fora period of several minutes, sequentially or substantiallysimultaneously with a solution of a cleaning formulation comprisingnitric acid and a detergent (e.g., a 1.5% solution) for a period ofseveral hours. The first stage may range from 1 hour to several hoursdepending on the amount and composition of the deposits to be removed,with longer times being used when a greater amount of deposited materialis present and/or when the deposited material is more difficult toremove. In some implementations, the cleaning formulation is added tothe process condensate pre-rinse for 4 minutes, sequentially orsubstantially simultaneously with a solution of a cleaning formulationcomprising nitric acid and a detergent (e.g., a 1.5% solution) for 6 to8 hours. In this example, pulse dosing is performed for 240 seconds (4minutes) every 360-480 minutes (6-8 hours). Stage 2 can comprise addinga lower concentration of the surfactant-based detergent cleaningformulation (e.g., 250 ppm) to the process condensate pre-rinse for aperiod of time (e.g., 4 minutes), sequentially or substantiallysimultaneously with (i) an organic deposit control formulation; and/or(ii) a cleaning formulation comprising nitric acid and a detergent for aperiod of time (e.g., 6 to 8 hours). The second stage may range from 1hour to several hours depending on the amount and composition of thedeposits to be removed. In one example, the organic deposit controlformulation is added in an amount to provide a concentration of 250 ppmfor 1 minute per hour, comprising two 30-second dosages (e.g., 4.5gallons/day or 135 gallons/month). In one example, the cleaningformulation comprising nitric acid and a detergent is a 1.0% solution.In some embodiments, such methods can be used for mash banks and heatexchangers and can be used every 12 to 15 hours.

In some embodiments, the first stage can comprise adding asurfactant-based detergent cleaning formulation to a process streamwherein, for example, the cleaning formulation is added to a processcondensate pre-rinse for 5 minutes in an amount to provide aconcentration of 500 ppm in the process condensate, sequentially orsubstantially simultaneously with a 1.5% solution of a cleaningformulation comprising nitric acid and a detergent for 1 hour (as aspray ball, in some embodiments). Stage 2 can comprise, for example,adding the surfactant-based detergent cleaning formulation to theprocess condensate pre-rinse for 5 minutes in an amount to provide aconcentration of 250 ppm, sequentially or substantially simultaneouslywith a 1.0% solution of a cleaning formulation comprising nitric acidand a detergent for 1 hour (as a spray ball, in some embodiments). Insome embodiments, such methods can be used for propagation and can beused every 12 to 15 hours.

In some embodiments, the first stage can comprise adding asurfactant-based detergent cleaning formulation to a process streamwherein, for example, the cleaning formulation is added to a processcondensate pre-rinse for 5 minutes in an amount to provide aconcentration of 500 ppm, sequentially or substantially simultaneouslywith a 1.5% solution of a cleaning formulation comprising nitric acidand a detergent for 1 hour (as a spray ball, in some embodiments) and a45-minute cooling. Stage 2 can comprise, for example, adding thesurfactant-based detergent cleaning formulation to the processcondensate pre-rinse for 5 minutes in an amount to provide aconcentration of 250 ppm, sequentially or substantially simultaneouslywith a 1.0% solution of a cleaning formulation comprising nitric acidand a detergent for 1 hour (as a spray ball, in some embodiments) and a45-minute cooling. In some embodiments, such methods can be used forfermenters and can be used every 12 to 15 hours.

In some embodiments, the first stage can comprise adding asurfactant-based detergent cleaning formulation to a process streamwherein, for example, the cleaning formulation is added to a processcondensate pre-rinse for 5 minutes in an amount to provide aconcentration of 500 ppm, sequentially or substantially simultaneouslywith a 1.5% solution of a cleaning formulation comprising nitric acidand a detergent for 45 minutes. Stage 2 can comprise, for example,adding the surfactant-based detergent cleaning formulation to theprocess condensate pre-rinse for 5 minutes in an amount to provide aconcentration of 250 ppm, sequentially or substantially simultaneouslywith a 1.0% solution of a cleaning formulation comprising nitric acidand a detergent for 45 minutes. In some embodiments, such methods can beused for fermenter fill headers and can be used every 48 hours perfermentation cycle.

In some embodiments, the first stage can comprise adding asurfactant-based detergent cleaning formulation to a process streamwherein, for example, the cleaning formulation is added to a processcondensate pre-rinse for 45 minutes in an amount to provide aconcentration of 1000 ppm, sequentially or substantially simultaneouslywith (i) a 1.5% solution of a cleaning formulation comprising nitricacid and a detergent for 4 hours; and/or (ii) a scale inhibitorformulation, which can be added in an amount to provide a concentrationof 20-30 ppm. Stage 2 can comprise, for example, adding thesurfactant-based detergent cleaning formulation to the processcondensate pre-rinse for 45 minutes in an amount to provide aconcentration of 500 ppm, sequentially or substantially simultaneouslywith (i) a 1.0% solution of a cleaning formulation comprising nitricacid and a detergent for 4 hours; (ii) an organic deposit controlformulation added for 1 minute per hour in an amount to provide aconcentration of 500 ppm, comprising two 30-second doses (e.g., 7.2gallons per day or 216 gallons per month); and/or (iii) a scaleinhibitor formulation, which can be added in an amount to provide aconcentration of 20-40 ppm. In some embodiments, such methods can beused for evaporators and can be used once per week.

In some embodiments, the first stage can comprise adding asurfactant-based detergent cleaning formulation to a process streamwherein, for example, the cleaning formulation is added to a processcondensate pre-rinse in an amount to provide a concentration of 1500ppm. Stage 2 can comprise adding 1000 ppm of the surfactant-baseddetergent cleaning formulation to the process condensate pre-rinse. Insome embodiments, such methods can be used for oil separation and can beused every 7-10 days.

Embodiments of the disclosed pulse dosing method provide advantages notrealized by continuous dosing methods with an equivalent concentrationof the cleaning formulation and/or methods in which no cleaningformulation is administered into the fluid process stream. As discussedherein, pulse dosing the cleaning formulation into a process streamcomprising corn, corn-derived products, or a combination thereof mayprovide smaller pressure increases and/or temperature drops through amash bank (heating and liquefaction unit) or heat exchanger compared tocontinuous dosing with an equivalent lower concentration of the cleaningformulation and/or methods relying solely on cleaning-in-process (CIP)at periodic intervals. And, as described herein, some embodiments of thepulse dosing method increase flow rates or provide smaller flow ratedecreases through separation screens of a fiber separation unit and/orprotein separation unit compared to continuous dosing into the processstream comprising corn, corn-derived products, or a combination thereofwith an equivalent lower concentration of the cleaning formulationand/or methods relying on periodic CIP only. Embodiments of thedisclosed pulse dosing method advantageously provide lower levels ofproduct contamination (e.g., ethanol and/or oil contamination withcleaning formulation components) compared to methods utilizingcontinuous dosing into the process stream comprising corn, corn-derivedproducts, or a combination thereof at effective levels, e.g., continuousdosing of the cleaning formulation to provide concentrations of 100 ppmor more. Additionally, the pulse dosing method may extendcleaning-in-process intervals requiring plant shutdowns for cleaningcompared to continuous dosing or no-dosing methods of operating theprocessing plant. For instance, CIP intervals may be increased 25%, 50%,75%, or even 100% or more when pulse dosing is used. In one example,cleaning intervals were increased from every 4-5 hours to every 8 hourswhen a cleaning formulation was administered using pulse dosing toscreens of a fiber separation unit. Cleaning during CIP events followingpulse dosing may be easier, requiring less effort, less intensivemethods, and/or less time than cleaning during CIP events followingcontinuous dosing with an equivalent lower concentration of the cleaningformulation and/or methods relying on periodic CIP only. Pulse dosingduring CIP events advantageously may shorten the CIP event and/or reducean amount of cleaning formulation required for effective cleaningcompared to a CIP process utilizing continuous dosing of the cleaningformulation.

IV. Formulations

Formulations that can be used in embodiments of the pulse dosing methoddisclosed herein can include surfactant-based detergent cleaningformulations (e.g., PHIBROCLEAN™) cleaning formulations comprisingnitric acid and a detergent (e.g., PHIBRO ACT™), scale inhibitorformulations (e.g., PHIBRO SI™), organic deposit control formulations(e.g., PHIBRO DC™), pH modifiers (e.g., acid, alkali, or a buffer), anoxidizer, a caustic solution, or any combination thereof. In someembodiments, the formulation is a nitric acid-containing formulation. Insuch embodiments, the nitric acid provides high strength dissolutionpower and the built-in detergent provides improved penetration of thecleaning solution into deposits and removal of organic scale components.Such formulations also are GRAS-compatible. And, such formulationembodiments are effective in dissolving and removing beer stone (e.g.,calcium and magnesium oxalate), calcium/magnesium phytate, struvite,combined organic/inorganic compounds, and combinations thereof. See, forexample, FIG. 3 as compared to FIG. 2 . Pulse dosing a nitricacid-containing formulation may reduce frequency and duration of CIPevents and/or reduce CIP chemical usage.

In some embodiments, the formulation is a detergent cleaner. Using suchformulations in pulse dosing methods can improve cleaning throughdetergent action, improve penetration of such solutions into depositsand assist in their removal, and provide potential savings in causticusage by facilitating the use of lower caustic concentrations andimproved caustic solution stability, extending intervals betweencleaning shutdowns, and combinations thereof. Also, such formulationsare Food Safety Modernization Act (FSMA) compliant. In some embodiments,such formulations can be added via pulse dosing to the fluid processstream remove organic material prior to a subsequent caustic CIP cycle,which can improve caustic solution stability and overall CIPeffectiveness, reduce frequency and duration of CIP events, and/orreduce CIP chemical usage. See, for example, FIG. 4 (detergent andcaustic) as compared to FIG. 5 (caustic only).

In yet additional embodiments, the formulation can be a scale inhibitor,which is effective in reducing formation of beer stone (e.g., calciumand magnesium oxalate), struvite, calcium and magnesium phytates,combined organic and inorganic deposits, and combinations thereof. Insome embodiments, scale formation can be reduced by thresholdinhibition, wherein pulse dosing modifies the chemistry of the fluidprocess stream to favor the formation of soluble compounds versusinsoluble compounds; sequestration, wherein the physical and chemicalinteraction of potential scale forming components is controlled,reducing scale formation reactions; and/or crystal modification, whichreduces the density of scale deposits that form, making them moreamorphous and less crystalline in nature and/or makes fouling that doesoccur easier to remove during subsequent cleaning events.

In yet some additional embodiments, the formulation can comprise anorganic deposit controlling formulation. Such embodiments can be pulsedosed directly into the process stream to control organic depositbuildup, can improve overall process consistency and performance, reducefrequency and duration of CIP events, and/or reduce CIP chemical usage.

Comparisons of various processing components (e.g., evaporator tubes)before and after treatment in a standard CIP process with a formulationof the present disclosure are shown in FIGS. 2 and 3 respectively. FIGS.4 and 5 show a comparison between a screen cleaned in a standard CIPprocess with a formulation of the present disclosure (FIG. 4 ) ascompared to using a caustic only (FIG. 5 ).

V. EXAMPLES Example 1

PhibroDC™ cleaning formulation was administered into a fluid processstream (corn mash) of an ethanol- and oil-processing plant at severallocations using pulse dosing. The PhibroDC™ cleaning formulation wasadministered into the mash bank for 60 seconds every 60 minutes toprovide a concentration of 250 ppm. FIG. 6 is a graph showing effects ofthe pulse dose administration on the ratio of pressure to flow rate overtime as the fluid process stream flowed from the mash bank to thefermentation unit. As shown in FIG. 6 , the pulsed dosing regimenreduced the pressure/flow ratio.

PhibroDC™ cleaning formulation was administered into the last evaporatorbefore oil recovery for 60 seconds per 60 minutes to provide aconcentration of 500 ppm. Typically, day-long hydroblasting is requiredto remove deposits and take apart the oil recovery stacked disc assemblyfor cleaning. However, following pulse dose administration of thecleaning formulation, deposited material on the discs began to peel offwithout hydroblasting (FIG. 7 ), and the assembly was easily separatedand cleaned with a standard pressure washer (FIG. 8 ).

The PhibroDC™ cleaning formulation was administered upstream of thesecondary and/or tertiary screens of the fiber separation unit via pulsedosing. The dosing was 500 ppm or 1000 ppm for 30 seconds every 30minutes. The effects on flow rate through the secondary screen withoutpulse dosing and at the two administered doses are shown in FIG. 9 andTable 1. The calculated ratios eliminate noise in the data. Results wereanalyzed using a one-way Anova test and student's t test. The differingconnecting letters indicate that the results are statisticallydifferent. Notably, the graph shows that there is less data indicating alow flow rate when the pulse dosing is used. Pulse dose administrationimproved the flow rate consistency. The connecting letters report showsthat the results are statistically different.

TABLE 1 Dose Std. Lower Upper Connecting (ppm) Mean Error 95% 95% letter0 0.890145 0.00025 0.88966 0.89063 A 500 0.907513 0.00019 0.907140.90789 B 1000 0.910233 0.00037 0.90951 0.91095 C

The effects on flow rate through the tertiary screen without pulsedosing and at the two administered doses are shown in FIG. 10 and Table2. Results were analyzed using a one-way Anova test and student's ttest. Notably, the graph shows that there is less data indicating a lowflow rate when the pulsed dosing is administered. The effects of pulseddosing at the tertiary screen is less pronounced since the flow rate isaffected also by flow through the primary and secondary screens.

TABLE 2 Dose (ppm) Mean Std. Error Lower 95% Upper 95% 0 0.8926070.00070 0.89123 0.89398 500 0.907109 0.00055 0.90604 0.90818 10000.916347 0.00105 0.91432 0.91843

FIG. 11 is a graph showing how flow rate typically varies over a 12-hourtimeframe in the absence of pulse dose administration of PhibroDC™cleaning formulation through the primary screen (ratio 1), secondaryscreen (ratio 2), tertiary screen (ratio 3), and overall (total ratio).The data shows significant decreases in flow rates between standardscreen cleanings (indicated by vertical arrows).

FIG. 12 is a comparable graph showing the effects of administeringpulsed doses of PhibroDC™ cleaning formulation on flow rate over timethrough the primary screen (ratio 1), secondary screen (ratio 2),tertiary screen (ratio 3), and overall (total ratio). The data in FIG.11 shows much less variability in flow rates and an increased intervalbetween standard screen cleanings. Pulse dose administration improvedthe flow rate consistency, largely eliminated low flow rate occurrences,and maintained stable flow ratios without flow rate decline betweenscreen washes.

Example 2

PhibroDC™ cleaning formulation was administered into a fluid processstream (corn mash) of an ethanol-processing plant using pulse dosing.The PhibroDC™ cleaning formulation was administered into the mash bankfor 30 seconds every 30 minutes to provide a concentration of 250 ppm inthe fluid process stream. The pressures were evaluated and normalized bythe flow rate. The linear regression of the pressure/flows vs. hours themash train was online was calculated for each cleaning cycle. Theresults are shown in FIGS. 13A and 13B. Advantageously, a smallerpressure increase over time resulted when the pulse dosing regimen wasused.

The temperature drop over time also was determined, and the linearregression of the beer-feed temperature over time was calculated foreach cleaning cycle. The results are shown in FIGS. 14A and 14B.Advantageously, a smaller temperature drop over time resulted when thepulse dosing regimen was used.

For comparison, the PhibroDC™ cleaning formulation was administeredcontinuously into the mash bank to provide a concentration of 4.2 ppm inthe fluid process stream. The 4.2 ppm continuous dose is an amount ofthe PhibroDC™ cleaning formulation that is equivalent to pulse dosingfor 60 seconds every 60 minutes (or 30 seconds every 30 minutes) toprovide a concentration of 250 ppm. The pressures were evaluated andnormalized by the flow rate. The linear regression of the pressure/flowsvs. hours the mash train was online was calculated for each cleaningcycle. The pressure effects are shown in FIGS. 15A and 15B.Surprisingly, continuous dosing at an equivalent lower dose had a slightnegative impact (higher dP/dt) compared to the baseline (no dose). Theresults are in stark contrast to the pulse dosing regimen results.

The temperature drop over time also was determined, and the linearregression of the beer-feed temperature over time was calculated. Theresults are shown in FIGS. 16A and 16B. Surprisingly again, continuousdosing had a negative impact (a larger dT/dt) compared to the baseline(no dose). In contrast, the pulse dosing regimen provided a clearadvantage over no dose.

The PhibroDC™ cleaning formulation was administered to the secondaryand/or tertiary screens of the fiber separation unit for 30 secondsevery 30 minutes to provide 500 ppm or 2000 ppm at the secondary screen.The results of administration to the secondary screen are shown in FIGS.17A-170 . Results were analyzed using a one-way Anova test, student'st-test, and Tukey-Kramer test. Addition of 500 ppm increased the meanratio from 89.94% to 90.56% (FIGS. 17A, 17B). Increasing the dosage to2000 ppm further increased the mean ratio as shown in FIG. 17C.

For comparison, the PhibroDC™ cleaning formulation was administeredcontinuously to the primary, secondary, and tertiary screens of thefiber separation unit to provide a concentration of 12 ppm in the fluidprocess stream. The 12 ppm continuous dose is an amount of the PhibroDC™cleaning formulation that is equivalent to pulse dosing for 60 secondsevery 60 minutes (or 30 seconds every 30 minutes) to provide aconcentration of 750 ppm. The results are shown in FIGS. 18A-18B(primary screen), 19A-19B (secondary screen), and 20A-20B (tertiaryscreen). Once again, the continuous dosing surprisingly had a slightnegative impact on flow through the separation screens compared to thebaseline (no dose). However, the pulse dosing regimen had a clearpositive impact (see e.g., FIG. 17A—pulse dosing vs. FIG. 19A—continuouslow dosing).

Example 3

A cleaning formulation is administered into a fluid process stream of aprocessing plant. The processing plant may be an ethanol processingplant, a protein processing plant, a corn oil processing plant, anethanol and protein processing plant, an ethanol and corn oil processingplant, or an ethanol, corn oil and protein processing plant, and thefluid process stream may be a corn mash stream. The cleaning formulationmay be pulse dosed into the fluid stream at one or more points of theprocessing plant, e.g., at a mash bank, a heat exchanger, an evaporator,or one or more separation screens of a separation unit. For comparison,an equivalent dose of the cleaning formulation is administeredcontinuously at the one or more points. For example, pulse dosing toprovide a concentration of 250 ppm, 500 ppm, 750 ppm, or 1000 ppm isperformed for 60 seconds every 60 minutes, or 30 seconds every 30minutes, and is compared to continuous dosing providing a concentrationof 4.2 ppm, 8.3 ppm, 12.5 ppm, or 16.7 ppm, respectively. Evaluatedparameters may include pressure, temperature, and/or flow rate overtime. It is expected that pulse dosing to a given concentration mayprovide superior results as evidenced by smaller pressure increases,smaller temperature drops, smaller flow rate drops, and/or greater flowrates over time compared to continuous dosing at an equivalent lowerconcentration of the cleaning formulation.

Example 4

Organic matter is baked onto one or more components to mimic depositsthat occur on processing plant components as the processing plant isoperated. For example, organic matter may be baked onto a separationscreen or an oil separator disc, or onto laboratory-sized components ofsimilar composition to components used in the processing plant. Thecomponents with baked-on organic matter are immersed continuously orintermittently in a fluid (e.g., a corn mash) containing a cleaningsolution. The components are immersed in fluids containing 250 ppm, 500ppm, 750 ppm, or 1000 ppm of the cleaning formulation for 30 secondsevery 30 minutes, or 60 seconds every 60 minutes, for a period of time.The period of time may be 2 hours, 4 hours, 6 hours, 8 hours, 12 hours,18 hours, or 24 hours. Components prepared the same way are continuouslyimmersed in fluids containing an equivalent dose, i.e., 4.2 ppm, 8.3ppm, 12.5 ppm, or 16.7 ppm cleaning formulation, respectively, for thesame period of time. Components also may be immersed in fluidscontaining no cleaning formulation for the same period of time. Thefluids may be maintained at a temperature similar to temperaturesemployed at the processing plant. When the period of time has elapsed,the components are evaluated. The amount of organic matter remaining onthe components is evaluated (e.g., visually) and the ease of removingthe organic matter is evaluated. Different cleaning methods, such aspressure washing, hydroblasting, cleaning with caustics, and/or othersuitable methods, are evaluated to compare the effects of pulse dosing,continuous dosing, and, optionally, no dosing. It is expected that pulsedosing may provide superior results as evidenced by easier cleaning ofcomponents subjected to pulse dosing to a given concentration comparedto components subjects to continuous immersion in fluids with anequivalent lower concentration of the cleaning formulation or in fluidswith no cleaning formulation.

In view of the many possible embodiments to which the principles of thepresent disclosure may be applied, it should be recognized that theillustrated embodiments are only preferred examples of the presentdisclosure and should not be taken as limiting. Rather, the scope of thepresent disclosure is defined by the following claims. I therefore claimas my invention all that comes within the scope and spirit of theseclaims.

I claim:
 1. A method, comprising cleaning a structural component of a processing facility by using pulse dosing to administer a cleaning formulation into a fluid process stream flowing through structural components of the processing facility, the fluid process stream comprising (i) corn, a corn-derived product, or a combination thereof, wherein the corn-derived product comprises a mash, whole stillage, or thin stillage, or (ii) a process condensate comprising water and other volatile components, a rinse fluid, a cleaning fluid, or a combination thereof, wherein pulse dosing comprises administering the cleaning formulation into the fluid process stream for a period of x seconds every y minutes, with no administration of the cleaning formulation between the periods of x seconds, wherein x and y independently are from 1 to
 500. 2. The method of claim 1, wherein x and y independently are from 5 to
 150. 3. The method of claim 1, wherein x=y.
 4. The method of claim 1, wherein x and y are different.
 5. The method of claim 1, wherein an amount of the cleaning formulation is administered into the fluid process stream to provide a concentration of 10 ppm to 50,000 ppm of the cleaning formulation in the fluid process stream during the period of x seconds.
 6. The method of claim 1, wherein the processing facility is an ethanol processing plant, a protein processing plant, a corn oil processing plant, an ethanol and corn oil processing plant, an ethanol and protein processing plant, or an ethanol, corn oil and protein processing plant.
 7. The method of claim 6, wherein the structural components of the processing facility are selected from a heating and liquefaction unit, a heat exchanger unit, a propagation unit, a fermentation unit, a distillation unit, an evaporation unit, a centrifuge unit, a fiber separation unit, a protein separation unit, an oil separation unit, or any combination thereof.
 8. The method of claim 7, wherein the cleaning formulation is administered into the fluid process stream at, or upstream of, at least one of the structural components.
 9. The method of claim 7, wherein the cleaning formulation is administered into the fluid process stream in, or upstream of, at least one of the heating and liquefaction unit, the heat exchanger unit, the evaporation unit, the fiber separation unit, the protein separation unit, the oil separation unit, or any combination thereof.
 10. The method of claim 7, wherein pulse dosing is performed for a period of x seconds every y minutes at each of at least two of the structural components, wherein at each of the at least two of the structural components, x and y independently are from 1 to
 500. 11. The method of claim 10, wherein an amount of the cleaning formulation administered into the fluid process stream at each of the at least two of the structural components independently provides a concentration of 10 ppm to 50,000 ppm of the cleaning formulation in the fluid process stream.
 12. The method of claim 10, wherein: (i) x=y at each one of the at least two of the structural components; or (ii) x and y at a first structural component of the at least two structural components are different than x and y, respectively, at a second structural component of the at least two structural components; or (iii) an amount of the cleaning formulation administered at a first structural component of the at least two of the structural components provides a different concentration of the cleaning formulation in the fluid process stream than an amount of the cleaning formulation administered at a subsequent structural component of the at least two of the structural components; or (iv) a chemical composition of the cleaning formulation administered at a first structural component of the at least two of the structural components is different than a chemical composition of the cleaning formulation administered at a subsequent structural component of the at least two of the structural components; or (v) any combination of two or more of (i), (ii), (iii), and (iv).
 13. The method of claim 7, wherein the fiber separation unit comprises one or more separation screens and the cleaning formulation is administered upstream of at least one of the one or more of the separation screens.
 14. The method of claim 13, wherein: the fiber separation unit comprises a primary separation screen, a secondary separation screen, and a tertiary separation screen; the cleaning formulation is administered via pulse dosing to the secondary separation screen to provide a first concentration of the cleaning formulation in the fluid process stream at or proximate the secondary separation screen; and the cleaning formulation is administered via pulse dosing to the tertiary separation screen to provide a second concentration of the cleaning formulation in the fluid process stream at or proximate to the tertiary separation screen.
 15. The method of claim 14, wherein the second concentration is less than the first concentration.
 16. The method of claim 7, wherein the fluid process stream comprises corn, corn-derived products, or a combination thereof, and wherein: (i) the cleaning formulation is administered into, or upstream of, the heating and liquefaction unit, and a mean pressure increase over time within the heating and liquefaction unit is smaller than a mean pressure increase over time when the cleaning formulation is not administered using pulse dosing; or (ii) the cleaning formulation is administered into, or upstream of, the heat exchange unit, and a mean pressure increase over time within the heat exchange unit is smaller than a mean pressure increase over time when the cleaning formulation is not administered using pulse dosing; or (iii) the cleaning formulation is administered into, or upstream of, the heating and liquefaction unit, and a mean temperature drop over time within the heating and liquefaction unit is smaller than a mean temperature drop over time when the cleaning formulation is not administered using pulse dosing; or (iv) the cleaning formulation is administered into, or upstream of, the heat exchanger unit, and a mean temperature drop over time within the heat exchanger unit is smaller than a mean temperature drop over time when the cleaning formulation is not administered using pulse dosing; or (v) the cleaning formulation is administered into, or upstream of, the fiber separation unit, and a mean flow rate over a period of time through the fiber separation unit is greater than a mean flow rate over the period of time through the fiber separation unit when the cleaning formulation is not administered using pulse dosing; or (vi) the cleaning formulation is administered into, or upstream of, the protein separation unit, and a mean flow rate over a period of time through the protein separation unit is greater than a mean flow rate over the period of time through the protein separation unit when the cleaning formulation is not administered using pulse dosing; or (vii) the cleaning formulation is administered into, or upstream of, the oil separation unit, and a mean flow rate over a period of time through the oil separation unit is greater than a mean flow rate over the period of time through the oil separation unit when the cleaning formulation is not administered using pulse dosing; or (viii) any combination of two or more of (i)-(vii).
 17. The method of claim 7, further comprising: ceasing flow of a first fluid process stream comprising corn, a corn-derived product, or a combination thereof through at least one of the structural components; initiating flow of a subsequent fluid process stream comprising the process condensate, rinse fluid, or combination thereof through the at least one of the structural components; and using pulse dosing to administer the cleaning formulation into the subsequent fluid process stream.
 18. The method of claim 17, wherein an amount of the cleaning formulation is administered into the subsequent fluid process stream to provide a concentration of 10 ppm to 50,000 ppm of the cleaning formulation in the subsequent fluid process stream during the period of x seconds.
 19. The method of claim 1, wherein the cleaning formulation comprises a detergent, a scale inhibitor, a pH modifier, an oxidizer, a caustic solution, or any combination thereof.
 20. A method of cleaning structural components of a processing facility, the method comprising cleaning the structural components of the processing facility by using pulse dosing to administer a cleaning formulation into a fluid process stream flowing through structural components of the processing facility using pulse dosing, wherein: the processing facility is an ethanol processing plant, a protein processing plant, a corn oil processing plant, an ethanol and protein processing plant, an ethanol and corn oil processing plant, or an ethanol, corn oil and protein processing plant; the fluid process stream comprises (i) corn, a corn-derived product, or a combination thereof, wherein the corn-derived product comprises a mash, whole stillage, or thin stillage, or (ii) a process condensate comprising water and other volatile components, a rinse fluid, a cleaning fluid, or a combination thereof; pulse dosing comprises administering the cleaning formulation into the fluid process stream for a period of x seconds every y minutes, with no administration of the cleaning formulation between the periods of x seconds; x and y independently are from 5 to 150; the cleaning formulation comprises a detergent, a scale inhibitor, a pH modifier, an oxidizer, a caustic solution, or any combination thereof; and an amount of the cleaning formulation is administered into the fluid process stream to provide a concentration of 10 ppm to 50,000 ppm of the cleaning formulation in the fluid process stream during the period of x seconds. 